Acetaldehyde → HCID 22258232, 화합물

HRID 1610833노트

반응식

HRID 1610833 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=O)[C:3]1=O.[C:10]([O-])(=O)[CH3:11].[NH4+:14].C(=O)C.[Cl-].[Na+].[NH3:20]>CS(C)=O>[CH3:11][C:10]1[NH:20][C:4]2[CH2:5][CH2:6][CH2:7][CH:2]([CH3:1])[C:3]=2[N:14]=1

참가 물질

7

반응물 5

HCID 177AcetaldehydeHCID 222AmmoniaHCID 5234Sodium ChlorideHCID 517165Ammonium AcetateHCID 33213603-Methylcyclohexane-1,2-dione

생성물 1

HCID 22258232HCID 22258232, 화합물수율 43.3%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

20.0 g (0.159 mol) of 3-Methyl-1,2-cyclohexanedione and 183.31 g (2.38 mol) of ammoniumacetate are dissolved in 760 ml DMSO. A solution of 27.94 g (0.34 mol) acetaldehyde dissolved in 40 ml DMSO is dropped to the reaction mixture. The reaction is heated for 20 minutes to 40° C., 20 minutes to 60° C. and 40 minutes to 80° C. The reaction is allowed to cool down to rt. 2.5 l saturated sodium chloride solution and ammonia are added to reach a pH of 8-9. The solution is extracted with ethyl acetate and the organic phases are dried over sodium sulfate. The solvent is evaporated under vacuum. The crystalls are filtrated and washed with ethyl acetate and diethyl ether to yield 10.3 g (43.3% of th.) 2,4-Dimethyl-4,5,6,7-tetrahydro-1H-benzimidazole.

후처리

  1. additionis dropped to the reaction mixture
  2. temperatureThe reaction is heated for 20 minutes to 40° C., 20 minutes to 60° C. and 40 minutes to 80° C
  3. extractionThe solution is extracted with ethyl acetate
  4. dry with materialthe organic phases are dried over sodium sulfate
  5. customThe solvent is evaporated under vacuum
  6. filtrationThe crystalls are filtrated
  7. washwashed with ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-f9765ab7993941fe9dd4be146d30532a
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06984646B2

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